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A practical multi-residue method based on ultra-performance liquid chromatography/tandem mass spectrometry was developed for the simultaneous determination of 23 perfluorinated alkylated substances (PFASs) in water and suspended particles. Suspended particle samples were extracted with 1% formic acid-acetonitrile and cleaned by matrix solid phase dispersion extraction using a C18 sorbent and graphitized carbon black. Water samples were filtered through 0.7-μm glass fiber membranes and enriched utilizing weak anion exchange cartridges. The eluent was dried under a gentle stream of N2 at 45°C and suspended in 1 mL acetonitrile-5 mM ammonium acetate (1:1, vol:vol). Gradient elution for chromatographic separation utilized acetonitrile and 5 mM ammonium acetate as mobile phases on a reverse phase C18 column. The compounds were quantified using an internal standard method in multiple reaction-monitoring mode. Limits of detection and quantitation of the 23 PFAS test compounds in water samples were 0.5-10 ng L−1 and 2-20 ng L-1, respectively. Recoveries at three fortified levels of 20, 50, and 200 ng L-1 ranged from 68.5% to 118% with relative standard deviations below 9.6%. We used this method to determine PFAS levels in real water and suspended particle samples and found high sensitivity and good reproducibility. [ABSTRACT FROM AUTHOR]

Atlantic blue fin tuna (Thunnus thynnus) is a species of great importance for Mediterranean Sea area, from both ecological and commercial points of view. The scientific literature reports few data on the contamination of this fish by emerging organic compounds such as perfluorinated alkylated substances (PFASs) and phthalates, being the latter never been studied in tuna. This study therefore investigated the presence of the PFASs perfluorooctane sulphonate (PFOS) and perfluoroctanoic acid (PFOA) and the phthalate di-2-ethylhexyl phthalate (DEHP), also monitored by its metabolite mono-2-ethylhexyl phthalate (MEHP), to assess both the state of contamination of Atlantic bluefin tuna specimen and the risk due to the toxicity of these compounds for human consumption. While PFOA was never found, detectable levels of PFOS (0.4-1.88 ng/g), DEHP (9-14.62 ng/g) and MEHP (1.5-6.30 ng/g) were found. The results were elaborated relating the accumulation to the size and age of the individuals and showed a correlation between the levels of different pollutants investigated. [ABSTRACT FROM AUTHOR]